反应详情

温度

85 °C

A 2.4 g portion of a dispersion containing 50% by weight of sodium hydride in a liquid paraffin was added in portions under an inert atmosphere to a solution containing 14.5 g (0.05 mole) 5,5-dimethyl-3-trimethoxysilylpropyl hydantoin and 150 cc of anhydrous N,N-dimethylformamide. The temperature of the reaction mixture was maintained at from 15° to 20° C. during the addition of the hydride. Following completion of the addition the mixture was stirred until hydrogen evolution ceased, at which time it was heated to 85° C., and 98.8 g of chloropropyltrimethoxysilane were added dropwise to the reaction mixture. A white precipitate formed as the addition progressed. Following completion of the addition the reaction mixture was heated at 95° C. for 16 hours, at which time the reaction mixture was cooled, filtered and the liquid phase distilled under reduced pressure to remove the N,N-dimethylformamide. The liquid paraffin was washed from the product using hexane. The identity of the residue as the expected silylhydantoin was confirmed using infra-red and nuclear magnetic resonance spectroscopy.

1. additionwas added in portions under an inert atmosphere to a solution
2. additioncompletion of the addition the mixture
3. customA white precipitate formed as the addition
4. additioncompletion of the addition the reaction mixture
5. temperaturewas heated at 95° C. for 16 hours, at which time the reaction mixture
6. temperaturewas cooled
7. filtrationfiltered
8. distillationthe liquid phase distilled under reduced pressure
9. customto remove the N,N-dimethylformamide
10. washThe liquid paraffin was washed from the product